CN106750165A - The preparation method of graphite polyurethane elastic composite - Google Patents

The preparation method of graphite polyurethane elastic composite Download PDF

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Publication number
CN106750165A
CN106750165A CN201611125433.5A CN201611125433A CN106750165A CN 106750165 A CN106750165 A CN 106750165A CN 201611125433 A CN201611125433 A CN 201611125433A CN 106750165 A CN106750165 A CN 106750165A
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China
Prior art keywords
graphite
degree
preparation
elastic composite
polyurethane elastic
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Pending
Application number
CN201611125433.5A
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Chinese (zh)
Inventor
王耀斌
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Shaanxi Gaoxin Industry Co Ltd
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Shaanxi Gaoxin Industry Co Ltd
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Priority to CN201611125433.5A priority Critical patent/CN106750165A/en
Publication of CN106750165A publication Critical patent/CN106750165A/en
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    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08GMACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G18/00Polymeric products of isocyanates or isothiocyanates
    • C08G18/06Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
    • C08G18/08Processes
    • C08G18/10Prepolymer processes involving reaction of isocyanates or isothiocyanates with compounds having active hydrogen in a first reaction step
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08GMACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G18/00Polymeric products of isocyanates or isothiocyanates
    • C08G18/06Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
    • C08G18/28Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
    • C08G18/40High-molecular-weight compounds
    • C08G18/48Polyethers
    • C08G18/4854Polyethers containing oxyalkylene groups having four carbon atoms in the alkylene group
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08GMACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G18/00Polymeric products of isocyanates or isothiocyanates
    • C08G18/06Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
    • C08G18/70Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the isocyanates or isothiocyanates used
    • C08G18/72Polyisocyanates or polyisothiocyanates
    • C08G18/74Polyisocyanates or polyisothiocyanates cyclic
    • C08G18/76Polyisocyanates or polyisothiocyanates cyclic aromatic
    • C08G18/7614Polyisocyanates or polyisothiocyanates cyclic aromatic containing only one aromatic ring
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/02Elements
    • C08K3/04Carbon

Abstract

The preparation method of graphite polyurethane elastic composite of the present invention is related to polyurethane industrial field, and in particular to the preparation method of graphite polyurethane elastic composite, comprises the following steps:The pretreatment of graphite, graphite 300g is taken in the beaker of 1000mL, add the absolute ethyl alcohol and stirring of 400mL uniform, graphite is fully dispersed in absolute ethyl alcohol, ultrasonically treated 30 min is carried out after standing 30 min, use Buchner funnel suction filtration, technique same as described above is repeated 3 times, and is then uniformly layered on iron pan, degree of being put into baking oven, taken out after 24 h, sample sack is loaded after cooling standby;The preparation of performed polymer, weigh graphite add there-necked flask in, then PTMG polyalcohol is added, after standing 12 h, the 3h of vacuum dehydration 2 under the conditions of 100 110 degree, cools to 50 60 degree, adds 2, the min of 4 one toluene di-isocyanate(TDI) low-temp reaction 50, is then warmed up to 80 85 degree of stirrings and the h of insulation reaction 3;The present invention is simple to operate, easy to process, and can guarantee that product quality, enhances product performance.

Description

The preparation method of graphite-polyurethane elastic composite
Technical field
The present invention relates to polyurethane industrial field, and in particular to the preparation method of graphite-polyurethane elastic composite.
Background technology
Polymer-layered fillers composite is the new material for developing rapidly in recent years, because it is except with general Beyond all of performance of logical composite, also with their unexistent advantages, such as heat resistance, barrier property and fire resistance Deng and cause the very big concern of scientific circles.For this respect research be concentrated mainly on enhancing to plastic material, toughness reinforcing and its Application and development in terms of mechanism.And layered fillers then reported in terms of elastic composite it is less.
Polyurethane elastomer (PUE) is the widely used polymeric material of a class, can be by progressively polymerization process Adjust its molecular chain structure or add organic and inorganic filler to improve its performance heart, such as pass through montmorillonite, silica, glass The filler modified PUE such as fiber.During with graphite as filler, existing report is concentrated mainly on preparation electric conductivity and thermally conductive materials.By Have in graphite and there is extremely strong bonded energy as clay-phase between layer structure, carbon atom, interlayer causes with aspect bonding force Various atoms, molecule, particle cluster can smoothly break through interlayer bonding force, insert interlayer, form compound between graphite layers, therefore, gather Urethane matrix carries out intercalation polymeric with graphite and can be prepared into graphite-PUE composites.This experiment is mainly made using cheap graphite It is filler, the preferable graphite-PUE composites of combination property is prepared for using prepolymer method, while having investigated content of graphite pair The influence of compound system performance.
The content of the invention
It is a kind of simple to operate present invention aim at providing, it is easy to process, and product quality is can guarantee that, enhance product performance Graphite-polyurethane elastic composite preparation method.
The preparation method of graphite-polyurethane elastic composite of the present invention, comprises the following steps:
The first step, the pretreatment of graphite
Graphite 300g is taken in the beaker of 1000mL, adds the absolute ethyl alcohol and stirring of 400mL uniform, graphite is fully dispersed in nothing In water-ethanol, ultrasonically treated 30 min is carried out after standing 30 min, uses Buchner funnel suction filtration, technique same as described above is repeated 3 times, Then uniformly it is layered on iron pan, degree of being put into baking oven, is taken out after 24 h, sample sack is loaded after cooling standby;
Second step, the preparation of performed polymer
Weigh in graphite addition there-necked flask, PTMG polyalcohol is then added, after standing 12 h, in 100- Vacuum dehydration 2-3h under the conditions of 110 degree, cools to 50-60 degree, adds the min of 2,4 one toluene di-isocyanate(TDI) low-temp reaction 50, Then the stirring of 80-85 degree and the h of insulation reaction 3 are warmed up to, the mass fraction of sampling analysis NCO bases is 5.58%, reaches design During nco value, i.e., performed polymer is prepared and finished, and sealing preserve is stand-by;
3rd step, the preparation of elastomer
Weighing performed polymer and being warmed up to 80-85 degree carries out a deaeration, plus people melts quantitative chain extender, and stirring 1-1.5min goes forward side by side After the secondary deaeration of row, pour into preheated mould, be put on vulcanizing press and vulcanized, curing temperature is 100 degree, 50 Mould unloading after min, then by sample cutting edge and after cure in an oven, after cure temperature is 100 degree, and the time is 15h, obtains final product stone Ink-polyurethane elastic composite.
Preferably, graphite is the graphite of the sheet of 500 mesh in the first step.
Preferably, chain extender is 3,3 '-two chloro- 4,4 '-two amido diphenyl-methanes.
The present invention is simple to operate, easy to process, and can guarantee that product quality, enhances product performance.
Specific embodiment
Embodiment one:
The preparation method of graphite-polyurethane elastic composite of the present invention, comprises the following steps:
The first step, the pretreatment of graphite
Graphite 300g is taken in the beaker of 1000mL, adds the absolute ethyl alcohol and stirring of 400mL uniform, graphite is fully dispersed in nothing In water-ethanol, ultrasonically treated 30 min is carried out after standing 30 min, uses Buchner funnel suction filtration, technique same as described above is repeated 3 times, Then uniformly it is layered on iron pan, degree of being put into baking oven, is taken out after 24 h, sample sack is loaded after cooling standby;
Second step, the preparation of performed polymer
Weigh in graphite addition there-necked flask, PTMG polyalcohol is then added, after standing 12 h, in 100- Vacuum dehydration 2-3h under the conditions of 110 degree, cools to 50-60 degree, adds the min of 2,4 one toluene di-isocyanate(TDI) low-temp reaction 50, Then the stirring of 80-85 degree and the h of insulation reaction 3 are warmed up to, the mass fraction of sampling analysis NCO bases is 5.58%, reaches design During nco value, i.e., performed polymer is prepared and finished, and sealing preserve is stand-by;
3rd step, the preparation of elastomer
Weighing performed polymer and being warmed up to 80-85 degree carries out a deaeration, plus people melts quantitative chain extender, and stirring 1-1.5min goes forward side by side After the secondary deaeration of row, pour into preheated mould, be put on vulcanizing press and vulcanized, curing temperature is 100 degree, 50 Mould unloading after min, then by sample cutting edge and after cure in an oven, after cure temperature is 100 degree, and the time is 15h, obtains final product stone Ink-polyurethane elastic composite.
Embodiment two:
The preparation method of graphite-polyurethane elastic composite of the present invention, comprises the following steps:
The first step, the pretreatment of graphite
Graphite 300g is taken in the beaker of 1000mL, adds the absolute ethyl alcohol and stirring of 400mL uniform, graphite is fully dispersed in nothing In water-ethanol, ultrasonically treated 30 min is carried out after standing 30 min, uses Buchner funnel suction filtration, technique same as described above is repeated 3 times, Then uniformly it is layered on iron pan, degree of being put into baking oven, is taken out after 24 h, sample sack is loaded after cooling standby;
Second step, the preparation of performed polymer
Weigh in graphite addition there-necked flask, PTMG polyalcohol is then added, after standing 12 h, in 100- Vacuum dehydration 2-3h under the conditions of 110 degree, cools to 50-60 degree, adds the min of 2,4 one toluene di-isocyanate(TDI) low-temp reaction 50, Then the stirring of 80-85 degree and the h of insulation reaction 3 are warmed up to, the mass fraction of sampling analysis NCO bases is 5.58%, reaches design During nco value, i.e., performed polymer is prepared and finished, and sealing preserve is stand-by;
3rd step, the preparation of elastomer
Weighing performed polymer and being warmed up to 80-85 degree carries out a deaeration, plus people melts quantitative chain extender, and stirring 1-1.5min goes forward side by side After the secondary deaeration of row, pour into preheated mould, be put on vulcanizing press and vulcanized, curing temperature is 100 degree, 50 Mould unloading after min, then by sample cutting edge and after cure in an oven, after cure temperature is 100 degree, and the time is 15h, obtains final product stone Ink-polyurethane elastic composite.
Graphite is the graphite of the sheet of 500 mesh in the first step.
Embodiment three:
The preparation method of graphite-polyurethane elastic composite of the present invention, comprises the following steps:
The first step, the pretreatment of graphite
Graphite 300g is taken in the beaker of 1000mL, adds the absolute ethyl alcohol and stirring of 400mL uniform, graphite is fully dispersed in nothing In water-ethanol, ultrasonically treated 30 min is carried out after standing 30 min, uses Buchner funnel suction filtration, technique same as described above is repeated 3 times, Then uniformly it is layered on iron pan, degree of being put into baking oven, is taken out after 24 h, sample sack is loaded after cooling standby;
Second step, the preparation of performed polymer
Weigh in graphite addition there-necked flask, PTMG polyalcohol is then added, after standing 12 h, in 100- Vacuum dehydration 2-3h under the conditions of 110 degree, cools to 50-60 degree, adds the min of 2,4 one toluene di-isocyanate(TDI) low-temp reaction 50, Then the stirring of 80-85 degree and the h of insulation reaction 3 are warmed up to, the mass fraction of sampling analysis NCO bases is 5.58%, reaches design During nco value, i.e., performed polymer is prepared and finished, and sealing preserve is stand-by;
3rd step, the preparation of elastomer
Weighing performed polymer and being warmed up to 80-85 degree carries out a deaeration, plus people melts quantitative chain extender, and stirring 1-1.5min goes forward side by side After the secondary deaeration of row, pour into preheated mould, be put on vulcanizing press and vulcanized, curing temperature is 100 degree, 50 Mould unloading after min, then by sample cutting edge and after cure in an oven, after cure temperature is 100 degree, and the time is 15h, obtains final product stone Ink-polyurethane elastic composite.
Graphite is the graphite of the sheet of 500 mesh in the first step.
Chain extender is 3,3 '-two chloro- 4,4 '-two amido diphenyl-methanes.
The present invention is simple to operate, easy to process, and can guarantee that product quality, enhances product performance.

Claims (3)

1. a kind of preparation method of graphite-polyurethane elastic composite, it is characterised in that comprise the following steps:
The first step, the pretreatment of graphite
Graphite 300g is taken in the beaker of 1000mL, adds the absolute ethyl alcohol and stirring of 400mL uniform, graphite is fully dispersed in nothing In water-ethanol, ultrasonically treated 30 min is carried out after standing 30 min, uses Buchner funnel suction filtration, technique same as described above is repeated 3 times, Then uniformly it is layered on iron pan, degree of being put into baking oven, is taken out after 24 h, sample sack is loaded after cooling standby;
Second step, the preparation of performed polymer
Weigh in graphite addition there-necked flask, PTMG polyalcohol is then added, after standing 12 h, in 100- Vacuum dehydration 2-3h under the conditions of 110 degree, cools to 50-60 degree, adds the min of 2,4 one toluene di-isocyanate(TDI) low-temp reaction 50, Then the stirring of 80-85 degree and the h of insulation reaction 3 are warmed up to, the mass fraction of sampling analysis NCO bases is 5.58%, reaches design During nco value, i.e., performed polymer is prepared and finished, and sealing preserve is stand-by;
3rd step, the preparation of elastomer
Weighing performed polymer and being warmed up to 80-85 degree carries out a deaeration, plus people melts quantitative chain extender, and stirring 1-1.5min goes forward side by side After the secondary deaeration of row, pour into preheated mould, be put on vulcanizing press and vulcanized, curing temperature is 100 degree, 50 Mould unloading after min, then by sample cutting edge and after cure in an oven, after cure temperature is 100 degree, and the time is 15h, obtains final product stone Ink-polyurethane elastic composite.
2. the preparation method of graphite-polyurethane elastic composite as claimed in claim 1, it is characterised in that in the first step Graphite is the graphite of the sheet of 500 mesh.
3. the preparation method of graphite-polyurethane elastic composite as claimed in claim 2, it is characterised in that the chain extension Agent is 3,3 '-two chloro- 4,4 '-two amido diphenyl-methanes.
CN201611125433.5A 2016-12-09 2016-12-09 The preparation method of graphite polyurethane elastic composite Pending CN106750165A (en)

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Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201611125433.5A CN106750165A (en) 2016-12-09 2016-12-09 The preparation method of graphite polyurethane elastic composite

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109810485A (en) * 2019-01-29 2019-05-28 天津百恩威新材料科技有限公司 Graphite/elastic resin composite grain, its preparation method and the application in production polishing wheel
CN110271073A (en) * 2019-05-13 2019-09-24 阜阳大可新材料股份有限公司 A kind of preparation method of 3D molded fiber plate

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109810485A (en) * 2019-01-29 2019-05-28 天津百恩威新材料科技有限公司 Graphite/elastic resin composite grain, its preparation method and the application in production polishing wheel
CN110271073A (en) * 2019-05-13 2019-09-24 阜阳大可新材料股份有限公司 A kind of preparation method of 3D molded fiber plate

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Application publication date: 20170531